CN112174996B - Method and device for continuously producing silane coupling agent - Google Patents
Method and device for continuously producing silane coupling agent Download PDFInfo
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- CN112174996B CN112174996B CN201910595085.5A CN201910595085A CN112174996B CN 112174996 B CN112174996 B CN 112174996B CN 201910595085 A CN201910595085 A CN 201910595085A CN 112174996 B CN112174996 B CN 112174996B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/122—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-C linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/14—Preparation thereof from optionally substituted halogenated silanes and hydrocarbons hydrosilylation reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a method for continuously producing a silane coupling agent, which comprises the following steps: the method is characterized in that hydrogen-containing silane and olefins are taken as raw materials, a catalyst is added, the raw materials are input into a reaction rectifying tower, and under the heating condition, the raw materials react in the reaction rectifying tower and are rectified and separated out to obtain a product, so that the continuous production of the silane coupling agent is realized. The invention also discloses a device for continuously producing the silane coupling agent, which comprises a first raw material tank, wherein the first raw material tank is provided with an olefin pipeline and a catalyst pipeline, and is used for mixing the catalyst and the olefin; a second raw material tank for holding hydrogen-containing silane; the reaction rectifying tower is connected with the first raw material tank and the second raw material tank, is used for reacting hydrosilane and olefins, and is used for rectifying and separating; and the product storage tank is connected with the tower kettle of the reaction rectifying tower and is used for storing target products. The invention can realize continuous production, improve the production efficiency of the silane coupling agent and promote the automatic production level.
Description
Technical Field
The invention belongs to the technical field of organic silicon, and particularly relates to a method and a device for continuously producing a silane coupling agent.
Background
The silane coupling agent is very important organic silicon, and because the molecule contains hydrophilic and lipophilic groups, the silane coupling agent can chemically react with synthetic resin or other polymers or generate hydrogen bonds, and is called as a 'molecular bridge', and is commonly used for improving the interface between inorganic matters and organic matters, so that the performance of the composite material is greatly improved. For example, the wear resistance and the aging resistance of products such as tires, rubber plates, rubber tubes and the like can be improved, and the use amount of rubber can be reduced.
In China, the consumption of organosilicon per person is far lower than that in developed countries, but the annual increase demand rate is kept at 5%, and the future market development space is huge. In addition, more and more foreign leading enterprises build factories in China, the rapid development of the downstream organic silicon industry in China is driven, and therefore, the demand for silane coupling agents is necessarily increasing.
However, the traditional method for preparing the silane coupling agent mostly adopts a batch method, has the defects of low production efficiency, high working strength and the like, is not suitable for large-scale production and application, and the yield of the silane coupling agent is difficult to meet the increasing market demand.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method and a device for continuously producing the silane coupling agent, which can realize continuous production, improve the production efficiency of the silane coupling agent and promote the automatic production level, aiming at the defects in the prior art.
The invention discloses a method for continuously producing a silane coupling agent, which is used for solving the technical problems, and the technical scheme is as follows:
a method for continuously producing a silane coupling agent comprises
Hydrogen-containing silane and olefins are taken as raw materials,
a catalyst is added in the reactor, and the catalyst is added in the reactor,
the raw materials are input into a reactive rectifying tower,
under the heating condition, the raw materials are rectified and separated out to obtain the product while reacting in a reaction rectifying tower, so that the continuous production of the silane coupling agent is realized.
Preferably, the method specifically comprises the following steps:
s1, pretreatment: firstly, uniformly mixing a catalyst and olefins, and then introducing the olefins mixed with the catalyst and hydrogen-containing silane into a reaction rectifying tower to uniformly mix the hydrogen-containing silane and the olefins mixed with the catalyst;
s2, reaction and rectification separation: heating the mixture in the reactive rectifying tower to the reaction temperature, enabling the hydrogen-containing silane and olefins to react under the action of a catalyst, rectifying and separating the products after the reaction in the process that the products enter a tower kettle, enabling the raw materials to react in the reactive rectifying tower while rectifying and separating the products, and outputting the products in the tower kettle to realize the continuous production of the silane coupling agent.
Preferably, the method further comprises step S3:
s3, reflux circulation: and conveying the materials in the tower bottom of the reaction rectifying tower to the tower top for reflux circulation, and gradually reducing the reflux ratio until the material system in the reaction rectifying tower is balanced and stably output, thereby realizing stable continuous production.
Preferably, the heating mode of the mixture in the reactive distillation column in step S2 is microwave heating.
Preferably, the reaction temperature of the mixture in the reactive distillation column in step S2 is 50-65 ℃.
Preferably, in the step S3, the reflux ratio of the materials in the bottom of the reaction rectifying tower when the output product is stable is as follows: 1.2 to 1.5.
Preferably, the hydrogen-containing silane is one of trichlorosilane and dichlorosilane;
the olefin is one of chloroethylene and chloropropene;
the catalyst is one of chloroplatinic acid and its complex.
Preferably, the molar ratio of the hydrogen-containing silane to the olefin is 1:1.2-1.5;
the catalyst is used as the total amount of the raw materials
According to the method for continuously producing the silane coupling agent, provided by the invention, microwaves and reactive distillation are combined, and the reaction rate can be accelerated through microwave radiation heating, so that the reaction period is greatly shortened; through the reaction rectifying tower, rectification separation is carried out while reaction is carried out, continuous production is realized, the yield and purity of the product are improved, the reaction heat is fully utilized in the rectification process, and the energy consumption is saved.
The invention discloses a device for continuously producing a silane coupling agent, which is used for solving the technical problems, and the technical scheme is as follows:
an apparatus for continuously producing a silane coupling agent, comprising:
a first feedstock tank provided with an olefin line and a catalyst line for mixing a catalyst and an olefin feedstock;
a second raw material tank for holding hydrogen-containing silane;
the reaction rectifying tower is connected with the first raw material tank and the second raw material tank, and is used for reacting hydrosilane and olefins under the action of a catalyst, and rectifying and separating;
and the product storage tank is connected with the tower kettle of the reaction rectifying tower and is used for storing target products.
Preferably, the heating device further comprises a heating device, wherein the heating device comprises a first heater and a second heater,
the first heater is arranged in the middle of the reaction rectifying tower and is used for heating materials in the middle of the reaction rectifying tower;
the second heater is arranged on the tower kettle of the reaction rectifying tower and is used for heating materials in the tower kettle of the reaction rectifying tower.
Preferably, the first heater is a microwave heater, and the second heater is a heat conducting oil heater.
Preferably, the circulating reflux mechanism further comprises a circulating pump and a circulating pipeline, wherein an inlet of the circulating pump is connected with the bottom of the tower kettle of the reaction rectifying tower, and an outlet of the circulating pump is connected with the top of the reaction rectifying tower and is used for conveying materials in the tower kettle to the top of the tower so as to realize reflux circulation.
Preferably, the first raw material tank and the second raw material tank are respectively connected with a first raw material pipeline and a second raw material pipeline, and are connected with the reaction rectifying tower through the first raw material pipeline and the second raw material pipeline, a first pump and a second pump are respectively arranged on the first raw material pipeline and the second raw material pipeline, and a distributor is arranged at one end of the first raw material pipeline and the second raw material pipeline extending into the reaction rectifying tower.
Preferably, the reactive distillation column further comprises a microwave suppressor and a liquid level gauge,
the microwave suppressor is arranged on the reaction rectifying tower and close to the tower kettle so as to prevent the microwave heater from heating the tower kettle;
the liquid level meter is arranged at the position of the tower kettle of the reaction rectifying tower and is used for detecting liquid level information in the tower kettle.
The device for continuously producing the silane coupling agent has the advantages of simple structure and convenient operation, can realize continuous production of the silane coupling agent, improves the production efficiency, avoids the problem of quality difference among batches during intermittent production, adopts single-loop automatic control on the reaction temperature and the rectification temperature in the running process of the device, reduces manual operation, controls the temperature more accurately, can reduce the byproduct production rate, and improves the product yield and purity.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus used in the method for continuously producing a silane coupling agent in example 1;
FIG. 2 is a schematic structural view of an apparatus used in the method for continuously producing a silane coupling agent in example 4.
In the figure: 1-a first raw material tank; 11-catalyst line; a 12-olefin line; 13-a stirrer; 14-a first pump; 15-a first flowmeter; 16 a first feed line; 2-a second feedstock tank; 21-a second pump; 22-a second flowmeter; 23-a second feed line; 3-a reactive rectifying tower; 31-a first thermometer; 32-a second thermometer; 33-a second heater; 34-tray; 35-a liquid level gauge; 4-a first heater; 5-a circulation pump; 51-a third flowmeter; 52-a circulation line; 53-fourth flow meter; 54-product line; 6-a product storage tank; 7-nitrogen line; 8, emptying the pipeline; 9-a pressure gauge; 10-distributor.
Detailed Description
In order to better understand the technical solution of the present invention, the present invention will be further clearly and completely described in the following with reference to the drawings and specific embodiments of the present invention.
In the prior art, the production process of the silane coupling agent has the defects of low production efficiency, high working strength and the like, is not suitable for large-scale production and application, and the yield of the silane coupling agent is difficult to meet the increasing market demand. Accordingly, the present invention provides a method for continuously producing a silane coupling agent, comprising
Hydrogen-containing silane and olefins are used as raw materials,
a catalyst is added in the reactor, and the catalyst is added in the reactor,
the raw materials are input into a reactive rectifying tower,
under the heating condition, the raw materials are rectified and separated out to obtain the product while reacting in a reaction rectifying tower, so as to realize the continuous production of the silane coupling agent.
Correspondingly, the invention also provides a device for continuously producing the silane coupling agent, which comprises:
a first feedstock tank provided with an olefin line and a catalyst line for mixing the catalyst and the olefin;
a second raw material tank for holding hydrogen-containing silane;
the reaction rectifying tower is connected with the first raw material tank and the second raw material tank, is used for reacting hydrosilane and olefins, and is used for rectifying and separating;
and the product storage tank is connected with the tower kettle of the reaction rectifying tower and is used for storing target products.
Example 1
As shown in fig. 1, this embodiment discloses an apparatus for continuously producing a silane coupling agent, comprising:
a first feedstock tank 1 provided with an olefin line 12 and a catalyst line 11 for mixing a catalyst and an olefin;
a second raw material tank 2 for holding hydrogen-containing silane;
the reaction rectifying tower 3 is connected with the first raw material tank and the second raw material tank, is used for reacting hydrosilane and olefins, and is used for rectifying and separating;
and the product storage tank 6 is connected with the tower kettle of the reaction rectifying tower and is used for storing target products.
The embodiment also discloses a method for continuously producing the silane coupling agent by using the device, which comprises the following steps:
hydrogen-containing silane and olefins are taken as raw materials,
a catalyst is added in the reactor, and the catalyst is added in the reactor,
the raw materials are input into a reactive rectifying tower,
under the heating condition, the raw materials are rectified and separated out to obtain the product while reacting in a reaction rectifying tower, so that the continuous production of the silane coupling agent is realized.
Wherein: the hydrogen-containing silane adopts one of trichlorosilane and dichlorosilane, the olefin adopts one of chloroethylene and chloropropene, and the mol ratio of the hydrogen-containing silane to the olefin is 1:1.2-1.5; the catalyst adopts one of chloroplatinic acid and its complex, and the dosage of the catalyst is the total amount of the raw materials
The method for continuously producing the silane coupling agent, namely the device, can realize continuous production of the silane coupling agent, improve the production efficiency, avoid the problem of quality difference among batches during intermittent production, improve the automation level in the production process, and is simple and feasible, reduces manual operation, ensures more accurate control, reduces the byproduct production rate, and improves the product yield and purity.
Example 2
This example discloses a method for continuously producing a silane coupling agent using the apparatus of example 1, which specifically comprises the steps of:
step S1: pretreatment of
Firstly, uniformly mixing a catalyst and olefins, then introducing the olefins mixed with the catalyst and hydrogen-containing silane into a reaction rectifying tower 3 to uniformly mix the hydrogen silane and the olefins mixed with the catalyst, and specifically comprising the following steps:
s101, purging equipment to remove oxygen;
specifically, nitrogen was introduced into all the equipment used in the method for continuously producing a silane coupling agent in this example to purge all the equipment (including the first raw material tank 1, the second raw material tank 2, the product tank 6, the reaction rectifying column 3, and connecting lines thereof), and oxygen in these equipment was discharged until the oxygen content was <1000ppm.
S102, preparing raw materials;
introducing a proper amount of olefins and a proper amount of catalysts into the first raw material tank, and stirring to uniformly mix the olefins and the catalysts; introducing a proper amount of hydrogen-containing silane into a second raw material tank;
wherein, the hydrogen-containing silane adopts one of trichlorosilane and dichlorosilane, and the trichlorosilane is preferable in the embodiment; the olefin is one of vinyl chloride and propylene chloride, and the preferred embodiment is vinyl chloride; the molar ratio of the hydrosilane to the olefins is 1:1.2-1.5, the preferred example is 1:1.2, i.e. the molar ratio of trichlorosilane to vinyl chloride is 1:1.2; the catalyst adopts one of chloroplatinic acid and its complex, and the dosage of the catalyst is the total amount of the raw materials
The catalyst of this example is preferably chloroplatinic acid in an amount of 4X10 based on the sum of the amounts of trichlorosilane and vinyl chloride -2 ％wt。
Specifically, trichlorosilane is respectively introduced into the second raw material tank, vinyl chloride is introduced into the first raw material tank according to the mol ratio of 1:1.2, and the total dosage of the trichlorosilane and the vinyl chloride is 4 multiplied by 10 -2 % wt. to the first feed tank, and stirring to mix the vinyl chloride and chloroplatinic acid catalyst uniformly.
S103, feeding;
introducing the olefin mixed with the catalyst and the hydrogen-containing silane into a reaction rectifying tower, and uniformly mixing the hydrogen-containing silane, the catalyst and the olefin raw materials.
Wherein, the position where the olefin mixed with the catalyst and the hydrosilane are introduced into the reactive distillation column 3 is the middle part or the top part of the reactive distillation column 3, and the embodiment is preferably the middle part of the reactive distillation column 3.
Specifically, the vinyl chloride mixed with the chloroplatinic acid catalyst in the first raw material tank is fed to the middle part of the reactive distillation column 3 through the first raw material line 16. Meanwhile, the trichlorosilane in the second raw material tank is conveyed to the middle part of the reaction rectifying tower 3 through the second raw material pipeline 23, and the two distributors 10 are oppositely arranged through the distributor 10 respectively arranged at the tail end of the first raw material pipeline 16 and the tail end of the second raw material pipeline 23, so that the chloroethylene mixed with the chloroplatinic acid catalyst and the trichlorosilane can be relatively and uniformly sprayed into the reaction rectifying tower 3 towards each other, and the chloroethylene mixed with the chloroplatinic acid catalyst and the trichlorosilane can be uniformly mixed and fully contacted.
Step S2: reaction and rectification separation
Heating the mixture in the reaction rectifying tower 3 to the reaction temperature, enabling hydrosilane and olefins to react under the action of a catalyst, rectifying and separating the reacted product in the process of entering a tower kettle, enabling the raw materials to react in the reaction rectifying tower 3 while rectifying and separating the product, and outputting the product in the tower kettle so as to realize the continuous production of the silane coupling agent. The heating mode in this embodiment is preferably microwave heating, and the reaction temperature is 50-65 ℃, and in this embodiment, 60 ℃.
S201, heating and reacting;
and heating the mixture in the reactive rectifying tower to a reaction temperature to enable the hydrosilane and olefins to react under the action of a catalyst to generate the silane coupling agent.
Specifically, the first heater 4 (in this embodiment, a microwave heater is preferable), microwaves generated by the microwave heater are fed from the middle part or the upper part of the reactive distillation column 3, preferably the middle part, and the mixture of trichlorosilane and vinyl chloride mixed with a chloroplatinic acid catalyst which has been fed into the reactive distillation column 3 is heated by the microwaves fed into the reactive distillation column 3, the mixture in the reactive distillation column 3 is heated to 60 ℃, and the reaction temperature is maintained, so that the trichlorosilane and the vinyl chloride react under the catalysis of the chloroplatinic acid to generate the silane coupling agent.
S202, rectifying and separating.
And rectifying and separating the reacted product in the tower kettle, so that the raw materials are rectified and separated out while reacting in the reaction rectifying tower, and the product is output in the tower kettle, thereby realizing the continuous production of the silane coupling agent.
Specifically, while trichlorosilane and chloroethylene are reacted under the catalytic action of chloroplatinic acid to produce a silane coupling agent, a second heater 33 (in the embodiment, a heat conducting oil heater is preferred) is started to heat the tower bottom of the reaction rectifying tower 3, so that a mixture (comprising trichlorosilane, chloroethylene, the silane coupling agent, si-O-Si and the like) in the tower bottom of the reaction rectifying tower 3 is gasified and ascended due to different boiling points, wherein light components (i.e. low-boiling-point substances such as trichlorosilane and chloroethylene) are gathered at the tower top, and heavy components (i.e. high-boiling-point substances such as silane coupling agent and Si-O-Si) are condensed and descended to the tower bottom, so that the high-boiling-point silane coupling agent is gradually separated and gathered at the tower bottom, and output to a product storage tank 3 in the tower bottom, thus a silane coupling agent product can be continuously obtained. In the process of ascending and descending of the light components, unreacted raw materials are fully contacted and continuously react to generate a silane coupling agent, so that the mixture of the reactive rectifying tower 3 is gradually and completely converted into the silane coupling agent after the rectification process in the process of entering the tower kettle, thereby improving the yield and purity of the silane coupling agent and realizing continuous production.
The detection shows that the yield of the silane coupling agent product is more than 90 percent and the purity is more than 99.9 percent.
Example 3
As shown in fig. 2, this embodiment discloses an apparatus for continuously producing a silane coupling agent, comprising:
a first feedstock tank 1 provided with an olefin line 12 and a catalyst line 11 for mixing a catalyst and an olefin;
a second raw material tank 2 for holding hydrogen-containing silane;
the reaction rectifying tower 3 is connected with the first raw material tank 1 and the second raw material tank 2 and is used for reacting hydrosilane and olefins and rectifying and separating;
and the product storage tank 6 is connected with the tower kettle of the reaction rectifying tower 3 and is used for storing target products.
Further, the first raw material tank 1, the second raw material tank 2, the reactive rectifying tower 3 and the product storage tank 6 are provided with a nitrogen pipeline 7, a pressure gauge 9 and a vent pipeline 8.
Specifically, a nitrogen line 7, a pressure gauge 9 and a vent line 8 are provided at the top of the reactive distillation column 3. Wherein: the nitrogen pipeline 7 is used for introducing nitrogen into the reactive distillation column 3 so as to purge the reactive distillation column 3 with nitrogen; the pressure gauge 9 is used for detecting the pressure in the reactive rectifying tower 3; the vent line 8 is used for discharging air of the reactive rectifying tower 3 during nitrogen purging so as to avoid adverse effects of oxygen in the air on the production process of the silane coupling agent. Furthermore, the vent pipeline 8 can be linked with the pressure gauge 9, and when the pressure value detected by the pressure gauge 9 is overlarge, the vent pipeline 8 is opened to release the pressure in the reactive rectifying tower 3, so that the safety of the production process is ensured.
The middle and lower parts in the reactive rectifying tower 3 are provided with the tower plates 34, the number of the tower plates 34 is preferably a plurality of multi-stage tower plates formed by the plurality of tower plates, so that better mass transfer and heat transfer effects can be achieved, unreacted raw materials are fully contacted in the gasification ascending or condensation descending process and react, the reaction is ensured to be more thorough, the rectifying and separating effect is improved, and the product yield and purity are improved.
Further, the first raw material tank 1 and the second raw material tank 2 are respectively connected with a first raw material pipeline 16 and a second raw material pipeline 23, and are connected with the reaction rectifying tower through the first raw material pipeline 16 and the second raw material pipeline 23, a first pump 14 and a second pump 21 are respectively arranged on the first raw material pipeline 16 and the second raw material pipeline 23, and a distributor 10 is arranged at one end of the first raw material pipeline 16 and the second raw material pipeline 23 extending into the reaction rectifying tower.
Specifically, an olefin pipeline 12 and a catalyst pipeline 11 are arranged at the top of the first raw material tank 1 and are respectively used for inputting olefin and catalyst into the first raw material tank; the first material tank 1 is further provided with a stirrer 13, and the stirrer 13 is preferably arranged to extend into the first material tank 1 from the top of the first material tank 1 and is used for stirring the olefins and the catalyst introduced into the first material tank 1 so as to ensure uniform mixing of the olefins and the catalyst. In this embodiment, the stirrer 13 is preferably a mechanical stirrer.
A first raw material line 16 is provided at the bottom of the first raw material tank 1, and the other end of the first raw material line 16 is connected to the middle or upper portion of the reactive distillation column 3, preferably to the middle portion of the reactive distillation column 3. A distributor 10 is provided at the end of the first feed line 16 extending into the reactive distillation column 3 in order to more evenly and dispersedly spray the catalyst-mixed olefins in the first feed tank 1 into the reactive distillation column 3. A first pump 14 and a first flowmeter 15 are arranged on the first raw material line, wherein: the first pump 14 is used for feeding the mixture of olefins and catalyst in the first feed tank 1 into the reactive rectifying column 3, and the first flowmeter 15 is used for detecting and controlling the input amount of olefins mixed with catalyst fed into the reactive rectifying column 3. In this embodiment, the first flowmeter 15 is preferably a mass flowmeter.
A nitrogen line 7, a pressure gauge 9 and a vent line 8 are provided at the top of the first raw material tank 1. Wherein: the nitrogen line 7 is used for introducing nitrogen into the first raw material tank 1 so as to purge the first raw material tank 1 and the first raw material line 16 with nitrogen; the pressure gauge 9 is used for detecting the pressure in the first raw material tank 1; the vent line 8 is used for exhausting air in the first raw material tank 1 during nitrogen purging so as to avoid adverse effect of oxygen in the air on the silane coupling agent production process. Further, the vent pipeline 8 can be linked with the pressure gauge 9, and when the pressure value detected by the pressure gauge 9 is too large, the vent pipeline 8 is opened to release the pressure in the first raw material tank 1, so that the safety of the production process is ensured.
Specifically, a second raw material line 23 is provided at the bottom of the second raw material tank 2, and the other end of the second raw material line 23 is connected to the middle or upper portion of the reactive distillation column 3, preferably to the middle portion of the reactive distillation column 3. A distributor 10 is provided at the end of the second raw material line 123 extending into the reactive rectifying column 3 so as to spray the hydrogen-containing silane in the second raw material tank 2 into the reactive rectifying column 3 more uniformly and dispersedly, and to be in full contact with and uniformly mix with the catalyst-mixed olefins introduced into the reactive rectifying column 3 from the first raw material tank 1. A second pump 21 and a second flowmeter 22 are arranged on the second raw material line 23, wherein: the second pump 21 is used for feeding the hydrogen-containing silane in the second raw material tank 2 into the reactive distillation column 3, and the second flowmeter 22 is used for detecting and controlling the feeding amount of the hydrogen-containing silane fed into the reactive distillation column 3. In this embodiment, the second flowmeter 21 is preferably a mass flowmeter.
A nitrogen line 7, a pressure gauge 9 and a vent line 8 are provided at the top of the second raw material tank 2. Wherein: the nitrogen line 7 is used for introducing nitrogen into the second raw material tank 2 so as to purge the second raw material tank 2 and the second raw material line 23 with nitrogen; the pressure gauge 9 is used for detecting the pressure in the second raw material tank 2; the vent line 8 is used for exhausting air in the second raw material tank 2 during nitrogen purging so as to avoid adverse effect of oxygen in the air on the production process of the silane coupling agent. Further, the vent pipeline 8 can be linked with the pressure gauge 9, and when the pressure value detected by the pressure gauge 9 is too large, the vent pipeline 8 is opened to release the pressure in the second raw material tank 2, so that the safety of the production process is ensured.
Further, the apparatus for continuously producing a silane coupling agent in this embodiment further comprises:
the circulating reflux mechanism comprises a circulating pump 5 and a circulating pipeline 52, wherein the inlet of the circulating pump is connected with the bottom of the tower kettle of the reactive distillation tower 3, and the outlet of the circulating pump is connected with the top of the reactive distillation tower 3 and is used for conveying materials in the tower kettle to the top of the tower so as to realize reflux circulation.
Specifically, an outlet is disposed at the bottom of the reactive distillation column 3 (i.e., the bottom of the column bottom), the outlet is connected with an inlet of the circulating pump 5, the outlet of the circulating pump 5 is connected with one end of the circulating pipeline 52, the other end of the circulating pipeline 52 is connected with the top of the reactive distillation column 3, and the circulating pump 5 is used for conveying the material in the column bottom to the top of the reactive distillation column 3 through the circulating pipeline 52 so as to perform total reflux or partial reflux. A third flowmeter 51 is provided on the circulation line 52, and the third flowmeter 51 is used for detecting an input amount of a material for reflux in a material in the column bottom. The outlet of the circulation pump 5 is also connected to the product tank 6 via a product line 54, and a fourth flow meter 53 is provided on the product line 54, the fourth flow meter 53 being used to detect the output of the product.
In this embodiment, by adjusting and controlling the ratio of the amount of the column bottom material for circulation to the amount of the produced product, that is, the reflux ratio, based on the detection results of the third flow meter 51, the fourth flow meter 53, a silane coupling agent of high purity can be obtained. In the present embodiment, the third flowmeter 51 and the fourth flowmeter 53 are preferably mass flowmeters.
Further, the apparatus for continuously producing a silane coupling agent in the present embodiment further comprises a heating device including a first heater 4 and a second heater 33, wherein: the first heater 4 is arranged in the middle of the reactive distillation column and is used for heating the reaction materials in the middle of the reactive distillation column; the second heater 33 is disposed on the tower bottom of the reactive distillation tower and is used for heating the material in the tower bottom of the reactive distillation tower.
Specifically, the first heater 4 is provided in the middle or upper part of the reactive distillation column 3, preferably in the middle. The first heater 4 is preferably a commercially available microwave heater having a function of setting a temperature and maintaining the set temperature (i.e., a constant temperature function), and the specific model is not further limited. The microwave heater can be provided with a required reaction temperature for heating the reaction rectifying tower 3 from the middle part of the reaction rectifying tower 3 so as to heat the reaction materials in the middle part of the reaction rectifying tower 3 to the required reaction temperature, and the working power of the microwave heater is regulated so as to maintain the reaction temperature unchanged, thereby realizing the accurate control of the reaction temperature and reducing the byproduct production rate.
In this embodiment, the frequency of the microwave heater is preferably 915MHZ, and the penetrating power of the microwave with this frequency is stronger, so that the material in the middle of the reactive rectifying tower 3 is heated more uniformly, and the reaction is more complete. The reaction temperature set on the microwave heater is preferably 50-65 ℃, that is to say the reaction temperature of the material in the reactive distillation column is preferably 50-65 ℃.
Further, a first thermometer 31 may be further disposed in the middle of the reactive rectifying tower 3, for monitoring and displaying the temperature of the material in the middle of the reactive rectifying tower 3 in real time.
Specifically, the second heater 33 is disposed on the bottom of the reactive distillation column 3, more precisely, on the outer wall of the bottom of the reactive distillation column 3. The second heater 33 is preferably a commercially available conduction oil heater having a function of setting a temperature and maintaining the set temperature (i.e., a constant temperature function), and the specific model is not further limited. The required temperature of the rectification separation process can be set on the heat conducting oil heater and is used for heating the tower kettle of the reaction rectifying tower 3 so as to control the temperature of the tower kettle of the reaction rectifying tower 3, so that the temperature of the tower kettle is maintained within the set required rectification temperature range, the rectification separation effect is improved, and the product yield and purity are improved.
In this embodiment, the temperature of the distillation set on the conduction oil heater is preferably 70-85 ℃, that is, the temperature of the distillation separation process is preferably 70-85 ℃.
Further, a second thermometer 32 may be further disposed on the tower bottom of the reactive rectifying tower 3, for monitoring and displaying the temperature of the material in the tower bottom of the reactive rectifying tower 3 in real time.
Further, the reactive rectifying column 3 further includes a microwave suppressor and a level gauge 35.
Specifically, the microwave suppressor is arranged at the position on the reaction rectifying tower 3, which is close to the tower kettle, and is used for preventing microwaves generated by the microwave heater from heating the tower kettle, so that the temperature of the tower kettle is difficult to control, the energy consumption loss is caused, and other byproducts can be reduced or avoided. The microwave suppressors in this embodiment are preferably materials having ultra-strong wave absorbing properties, such as ferrite, graphite, etc., that is, ferrite or graphite materials are installed on the reaction rectifying column 3 at a position close to the column bottom. The liquid level meter 35 is arranged at the tower kettle position of the reactive rectifying tower 3 and is used for detecting liquid level information in the tower kettle so as to control feeding and extracting products.
The device for continuously producing the silane coupling agent in the embodiment, the process for producing the silane coupling agent is described in detail as follows:
(1) Nitrogen is input through a nitrogen pipeline 7, all equipment such as the reactive rectifying tower 3 and the like are purged, and oxygen in the equipment is discharged from a vent pipeline 8 until the oxygen content is less than 1000ppm;
(2) The olefin is input into the first raw material tank 1 through the olefin pipeline 12, the catalyst is input into the first raw material tank 1 through the catalyst pipeline 11, and the stirrer 13 is started to uniformly mix the olefin and the catalyst; at the same time, hydrogen-containing silane is fed into the second raw material tank 2;
(3) Starting a microwave heater while introducing raw materials into the reaction rectifying tower 3, heating the reaction rectifying tower 3 to 50-65 ℃, simultaneously starting a first pump 14 and a second pump 21, respectively conveying olefin mixed with a catalyst and hydrogen-containing silane to the reaction rectifying tower 3, spraying the olefin mixed with the catalyst and the hydrogen-containing silane into the reaction rectifying tower through a distributor 10, uniformly mixing the olefin mixed with the catalyst and the hydrogen-containing silane, fully contacting, and reacting;
(4) Starting a heat conduction oil heater while starting a microwave heater, heating the tower kettle to 70-85 ℃, and performing total reflux at the initial stage of the reaction (namely, microwave heating for 0-60 min), namely, conveying the materials of the tower kettle to the tower top through a circulating pump, and continuing the reaction;
(5) After the material system in the reactive rectifying tower 3 is stable, a part of the material in the tower kettle is refluxed by adjusting the reflux ratio, and the other part is extracted as a product and is conveyed to a product storage tank 6 for standby by a circulating pump 5, so that continuous production is realized.
The device for continuously producing the silane coupling agent disclosed by the embodiment has the advantages that the structure is simple, the operation is convenient, the continuous production of the silane coupling agent can be realized, the production efficiency is improved, the problem of quality difference among batches during intermittent production is avoided, in the running process of the device, the reaction temperature and the rectification temperature are automatically controlled by adopting a single loop, the manual operation is reduced, the temperature is controlled more accurately, the byproduct production rate can be reduced, and the product yield (which can reach 90-95% through detection) and the purity (which can reach 99.5% -99.5% through detection) are improved.
Example 4
This example discloses a method for continuously producing a silane coupling agent using the apparatus of example 3, which specifically comprises the steps of:
step S1: pretreatment stage
The catalyst and the olefin are uniformly mixed, and then the olefin mixed with the catalyst and the hydrosilane are introduced into the reaction rectifying tower 3, so that the hydrosilane and the olefin mixed with the catalyst are uniformly mixed.
S101, purging equipment to remove oxygen;
specifically, nitrogen was introduced into all the equipment used in the method for continuously producing a silane coupling agent in this example to purge all the equipment (including the first raw material tank 1, the second raw material tank 2, the product tank 6, the reaction rectifying column 3, and connecting lines thereof), and oxygen in these equipment was discharged until the oxygen content was <1000ppm.
S102, preparing raw materials;
introducing a proper amount of olefins and a proper amount of catalysts into the first raw material tank, and stirring to uniformly mix the olefins and the catalysts; introducing a proper amount of hydrogen-containing silane into a second raw material tank;
wherein, the hydrogen-containing silane adopts one of trichlorosilane and dichlorosilane, and the dichlorosilane is preferable in the embodiment; the olefin is one of vinyl chloride and chloropropene, and the preferred embodiment is chloropropene; the molar ratio of the hydrosilane to the olefins is 1:1.2-1.5, the preferred example is 1:1.5, i.e. the molar ratio of dichlorosilane to chloropropene is 1:1.5; the catalyst adopts one of chloroplatinic acid and its complex, and the dosage of the catalyst is the total amount of the raw materials
The catalyst of this example is preferably a chloroplatinic acid complex in an amount of 6X 10 based on the sum of the amounts of dichlorosilane and chloropropene -2 ％wt。
Specifically, dichlorosilane is respectively introduced into the second raw material tank, chloropropionenes are introduced into the first raw material tank according to the mol ratio of 1:1.5, and the total dosage of the dichlorosilane and chloropropene is 6 multiplied by 10 -2 % wt. to the first feed tank, chloroplatinic acid complex as catalyst was introduced and stirredThe chloropropion olefin and the chloroplatinic acid complex catalyst are uniformly mixed.
S103, feeding;
introducing the olefin mixed with the catalyst and the hydrosilane into a reaction rectifying tower, and uniformly mixing the hydrosilane, the catalyst and the olefin.
Wherein, the position where the olefin mixed with the catalyst and the hydrosilane are introduced into the reactive distillation column 3 is the middle part or the top part of the reactive distillation column 3, and the embodiment is preferably the middle part of the reactive distillation column 3.
Specifically, the chloropropene mixed with the chloroplatinic acid complex catalyst in the first raw material tank is conveyed to the middle part of the reactive distillation column 3 through the first raw material line 16. Meanwhile, the dichlorosilane in the second raw material tank is conveyed to the middle part of the reactive rectifying tower 3 through the second raw material pipeline 23, and the two distributors 10 are oppositely arranged through the distributor 10 respectively arranged at the tail end of the first raw material pipeline 16 and the tail end of the second raw material pipeline 23, so that the chloropropene and the dichlorosilane mixed with the chloroplatinic acid complex catalyst can be relatively and uniformly sprayed into the reactive rectifying tower 3 towards each other, and the chloropropene and the dichlorosilane mixed with the chloroplatinic acid complex catalyst can be uniformly mixed and fully contacted.
Step S2: reaction and rectification separation stage
Heating the mixture in the reaction rectifying tower 3 to the reaction temperature, enabling hydrosilane and olefins to react under the action of a catalyst, rectifying and separating the reacted product in the process of entering a tower kettle, enabling the raw materials to react in the reaction rectifying tower 3 while rectifying and separating the product, and outputting the product in the tower kettle so as to realize the continuous production of the silane coupling agent.
The heating mode in this embodiment is preferably microwave heating, and the reaction temperature is 50-65 ℃, and in this embodiment, it is preferably 65 ℃.
S201, heating and reacting;
and heating the mixture in the reactive rectifying tower to a reaction temperature to enable the hydrosilane and olefins to react under the action of a catalyst to generate the silane coupling agent.
Specifically, the first heater 4 (in this embodiment, a microwave heater is preferable), microwaves generated by the microwave heater are fed from the middle part or the upper part of the reactive distillation column 3, preferably the middle part, the mixture which has been fed into the reactive distillation column 3 is heated by the microwaves fed into the reactive distillation column 3, the mixture in the reactive distillation column 3 is heated to 65 ℃, and the reaction temperature is maintained, so that dichlorosilane and chloropropene mixed with a chloroplatinic acid complex catalyst are reacted to produce a silane coupling agent.
S202, rectifying and separating.
And rectifying and separating the reacted product in the tower kettle, so that the raw materials are rectified and separated out while reacting in the reaction rectifying tower, and the product is output in the tower kettle, thereby realizing the continuous production of the silane coupling agent.
Specifically, while trichlorosilane and chloropropene react under the catalytic action of chloroplatinic acid to produce a silane coupling agent, a second heater 33 (in the embodiment, a heat conducting oil heater is preferred) is started to heat the tower bottom of the reaction rectifying tower 3, so that a mixture (comprising trichlorosilane, chloropropene, the silane coupling agent, si-O-Si and the like) in the tower bottom of the reaction rectifying tower 3 is gasified and raised due to different boiling points, light components (i.e. low-boiling-point substances such as trichlorosilane and chloropropene) in the mixture are gathered at the tower top, and heavy components (i.e. high-boiling-point substances such as silane coupling agent and Si-O-Si) are condensed and lowered to be gathered at the tower bottom, so that the high-boiling-point silane coupling agent is gradually separated and gathered at the tower bottom, and output to a product storage tank 3 in the tower bottom, and thus a silane coupling agent product can be continuously obtained. In the process of ascending and descending of the light components, unreacted raw materials are fully contacted and continuously react to generate a silane coupling agent, so that the mixture of the reactive rectifying tower 3 is gradually and completely converted into the silane coupling agent after the rectification process in the process of entering the tower kettle, thereby improving the yield and purity of the silane coupling agent and realizing continuous production.
In this embodiment, it is considered that most of the materials are not fully reacted at the initial stage of the reaction, and the silane coupling agent produced by the reaction is small, and the yield and purity of the product are low. Therefore, the materials at the bottom of the reactive rectifying tower 3 are conveyed to the top of the reactive rectifying tower 3 at the initial stage of the reaction, and reflux is carried out, so that the yield is improved.
Further, the method for continuously producing the silane coupling agent in the embodiment further comprises,
step 3: reflux circulation
And (3) conveying the materials in the tower bottom of the reaction rectifying tower 3 to the tower top for reflux circulation, wherein the reflux circulation ratio is gradually reduced from large to small until the material system in the reaction rectifying tower is balanced and stably output (the condition that the material system is stable, namely the purity of the silane coupling agent in the materials output by the tower bottom reaches the extraction requirement, in the embodiment, the purity of the silane coupling agent reaches 99.5 percent), so that stable continuous production is realized.
S301, total reflux;
in the initial stage of the reaction, all materials in the tower bottom of the reaction rectifying tower 3 are conveyed to the top of the reaction rectifying tower 3 for total reflux.
The initial stage of the reaction is just when the microwave heating is started, preferably the microwave heating time is 0 to 60min, and in this embodiment, the microwave heating is preferably performed for 60 min.
Specifically, materials in the tower bottom of the reaction rectifying tower 3 are all conveyed to the tower top of the reaction rectifying tower 3 through a circulating pipeline by utilizing a circulating pump within the first 60min of microwave heating, so that unreacted materials in the materials are fully contacted and heat-exchanged again, and the materials continue to react to generate a silane coupling agent, so that the materials are continuously circulated, and the reaction is more complete.
In this embodiment, the total reflux is performed in the early reaction stage (i.e., within 0-60min of microwave heating), so that the materials in the reactive distillation column 3 can fully react, the material system in the reactive distillation column 3 can be quickly stabilized (the stable condition of the material system, i.e., the purity of the silane coupling agent in the materials output from the column bottom, reaches the extraction requirement, in this embodiment, the purity of the silane coupling agent reaches 99.5%), the non-production time period is shortened, and the production efficiency is improved.
S202, partially refluxing and separating a product;
after the material system of the reactive rectifying tower 3 is stable, outputting a product, and adjusting a reflux ratio (in the embodiment, the reflux ratio refers to the weight ratio of the material L which is refluxed to the top part of the tower and the material D which is the output product, namely R=L/D), so that part of the tower material continuously refluxes, and the other part of the tower material is continuously extracted from the bottom of the reactive rectifying tower 3 as the product and is output to a product storage tank 6, thereby realizing continuous production and obtaining the high-purity silane coupling agent.
Wherein, the reflux ratio of the materials in the kettle of the reaction rectifying tower 3 is 1.2-1.5 when the products are stably output, and the preferred embodiment is 1.2.
Specifically, when the purity of the silane coupling agent in the material in the tower kettle in the reaction rectifying tower 3 reaches 99.5%, the reflux ratio is adjusted to be 1.2, so that one part of the tower kettle material continuously flows back to the tower top, and the other part of the tower kettle material is continuously extracted from the bottom of the reaction rectifying tower 3 as a product and is output to a product storage tank 6, continuous production is realized, and the high-purity silane coupling agent is obtained.
Through detection, the yield of the silane coupling agent product is more than 90 percent, and the purity is more than 99.5 percent.
According to the method for continuously producing the silane coupling agent, disclosed by the embodiment, microwaves and reactive distillation are combined, and the reaction rate can be accelerated through microwave radiation heating, so that the reaction period is greatly shortened; through the reaction rectifying tower, rectification separation is carried out while reaction is carried out, continuous production is realized, the yield and purity of the product are improved, the reaction heat is fully utilized in the rectification process, and the energy consumption is saved.
It is to be understood that the foregoing description is only of the preferred embodiments of the invention, however, the invention is not limited thereto. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (9)
1. A method for continuously producing a silane coupling agent, comprising:
hydrogen-containing silane and olefins are taken as raw materials,
a catalyst is added in the reactor, and the catalyst is added in the reactor,
the raw materials are input into a reactive rectifying tower,
under the heating condition, the raw materials are rectified and separated out to obtain a product while reacting in a reaction rectifying tower, so that the continuous production of the silane coupling agent is realized;
the hydrogen-containing silane is one of trichlorosilane and dichlorosilane;
the olefin is one of chloroethylene and chloropropene;
the catalyst is one of chloroplatinic acid and complex thereof;
the position of the raw material which is introduced into the reaction rectifying tower is the middle part or the top part of the reaction rectifying tower, and the heating conditions are that the middle part or the upper part of the reaction rectifying tower is heated to 50-65 ℃ by a first heater, and the tower bottom of the reaction rectifying tower is heated by a second heater so as to control the temperature of the tower bottom of the reaction rectifying tower, so that the temperature of the tower bottom is maintained at the rectifying temperature of 70-85 ℃;
the method specifically comprises the following steps:
s1, pretreatment: firstly, uniformly mixing a catalyst and olefins, and then introducing the olefins mixed with the catalyst and hydrogen-containing silane into a reaction rectifying tower to uniformly mix the hydrogen-containing silane and the olefins mixed with the catalyst;
s2, reaction and rectification separation: heating the mixture in the reaction rectifying tower to the reaction temperature, enabling hydrosilane and olefins to react under the action of a catalyst, rectifying and separating the reacted product in the process that the product enters a tower kettle, enabling the raw materials to react in the reaction rectifying tower while rectifying and separating the product, and outputting the product in the tower kettle to realize the continuous production of the silane coupling agent;
in step S2, the mixture in the reactive distillation column is heated by microwaves.
2. The method for continuously producing a silane coupling agent according to claim 1, further comprising step S3:
s3, reflux circulation: and conveying the materials in the tower bottom of the reaction rectifying tower to the tower top for reflux circulation, and gradually reducing the reflux ratio until the material system in the reaction rectifying tower is balanced and stably output, thereby realizing stable continuous production.
3. The method for continuously producing a silane coupling agent according to claim 1, wherein the reaction temperature of the mixture in the reactive distillation column in step S2 is 50 to 65 ℃.
4. The method for continuously producing a silane coupling agent according to claim 2, wherein in the step S3, the reflux ratio of the materials in the bottom of the reaction rectifying column at the time of stable output of the product is: 1.2 to 1.5.
5. The method for continuously producing a silane coupling agent according to claim 1, wherein,
the molar ratio of the hydrogen-containing silane to the olefin is 1:1.2-1.5;
the dosage of the catalyst is 4x10 of the total amount of the raw materials -2 %wt～6x10 -2 %wt。
6. An apparatus for continuously producing a silane coupling agent, comprising:
a first raw material tank (1) provided with an olefin line (12) and a catalyst line (11) for mixing a catalyst and an olefin raw material;
a second raw material tank (2) for holding hydrogen-containing silane;
the reaction rectifying tower (3) is connected with the first raw material tank and the second raw material tank and is used for reacting hydrosilane and olefins under the action of a catalyst and rectifying and separating, wherein the first raw material tank and the second raw material tank are respectively connected with a first raw material pipeline (16) and a second raw material pipeline (23), the other end of the first raw material pipeline is connected with the middle part or the upper part of the reaction rectifying tower, and the other end of the second raw material pipeline is connected with the middle part or the upper part of the reaction rectifying tower;
a product storage tank (6) connected with the tower bottom of the reaction rectifying tower and used for storing target products;
a heating device comprising a first heater (4) and a second heater (33),
the first heater is arranged at the middle part or the upper part of the reaction rectifying tower and is used for heating the material at the middle part of the reaction rectifying tower,
the second heater is arranged on the tower kettle of the reaction rectifying tower and is used for heating materials in the tower kettle of the reaction rectifying tower;
the first heater is a microwave heater, and the second heater is a heat conduction oil heater.
7. The apparatus for continuously producing silane coupling agent according to claim 6, further comprising a circulating reflux mechanism comprising a circulating pump and a circulating line, wherein an inlet of the circulating pump is connected with a bottom of a column bottom of the reactive distillation column, and an outlet thereof is connected with a top of the reactive distillation column for transporting a material in the column bottom to the top of the column to realize a reflux cycle.
8. The apparatus for continuously producing a silane coupling agent according to claim 6, wherein a first pump (14) and a second pump (21) are provided on the first raw material line and the second raw material line, respectively, and a distributor (10) is provided on each of the ends of the first raw material line and the second raw material line extending into the reactive rectifying column.
9. The apparatus for continuously producing a silane coupling agent according to claim 6, wherein the reactive distillation column further comprises a microwave suppressor and a level gauge (35),
the microwave suppressor is arranged on the reaction rectifying tower and close to the tower kettle so as to prevent the microwave heater from heating the tower kettle;
the liquid level meter is arranged at the position of the tower kettle of the reaction rectifying tower and is used for detecting liquid level information in the tower kettle.
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| CN101511732A (en) * | 2006-09-27 | 2009-08-19 | 电气化学工业株式会社 | Process for continuously producing monosilane |
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| CN101139354A (en) * | 2006-08-10 | 2008-03-12 | 德古萨有限责任公司 | System and process for continuous industrial preparation of 3-chloropropylchlorosilanes |
| CN101511732A (en) * | 2006-09-27 | 2009-08-19 | 电气化学工业株式会社 | Process for continuously producing monosilane |
| CN109482117A (en) * | 2018-11-13 | 2019-03-19 | 江西宏柏新材料股份有限公司 | The device and method of atmospheric distillation reaction production cyanoethyl alkoxy silane |
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